1, njirimara nke usoro hydroxypropyl methyl cellulose
(1) Were 1.0g nke sample, kpụ ọkụ n'ọnụ mmiri (80 ~ 90 ℃) 100mL, nwuo nọgidere, na jụụ n'ime viscous mmiri mmiri na ice saa; Tinye 2ml nke mmiri mmiri n'ime tube ule, jiri nwayọọ nwayọọ tinye 1mL sulfuric acid ngwọta nke 0.035% anthrone n'akụkụ mgbidi tube, ma hapụ maka 5min. Mgbanaka akwụkwọ ndụ akwụkwọ ndụ na-egosi na interface dị n'etiti mmiri mmiri abụọ ahụ.
(2) Were ego kwesịrị ekwesị nke slime ahụ a kpọtụrụ aha n'elu nke ejiri na njirimara (ⅰ) ma wụsa ya na efere ugegbe. Mgbe mmiri ahụ kwụsịrị, a na-emepụta ihe nkiri ductile.
2, hydroxypropyl methyl cellulose analysis nke ọkọlọtọ ngwọta nkwadebe
(1) Sodium thiosulfate ọkọlọtọ ngwọta (0.1mol/L, irè: otu ọnwa)
Nkwadebe: Obụpde banyere 1500mL distilled mmiri na jụụ ruo mgbe njikere iji. Tulee 25g sodium thiosulfate (ihe dị arọ ya bụ 248.17, ma gbalịa ka ọ bụrụ ihe dị ka 24.817g mgbe ị na-atụ aro) ma ọ bụ 16g sodium thiosulfate anhydrous, gbazee ya na 200ml nke mmiri jụrụ oyi n'elu, gbanye ya na 1L, tinye ya na aja aja. karama, tinye karama ahụ n'ọchịchịrị, ma kpochaa ya maka ojiji mgbe izu abụọ gachara.
Nhazi: tụọ 0.15g ntụaka potassium dichromate butere na ịdị arọ mgbe niile, ziri ezi na 0.0002g. Tinye 2g potassium iodide na 20mL sulfuric acid (1+9), maa jijiji nke ọma, tinye n'ime ọchịchịrị maka 10min, tinye 150ml mmiri na 3ml 0.5% starch egosi ngwọta, titrate na 0.1mol/L sodium thiosulfate ngwọta, ngwọta na-atụgharị site na-acha anụnụ anụnụ. ka akwụkwọ ndụ akwụkwọ ndụ na-egbuke egbuke na njedebe njedebe. E tinyeghị potassium chromate na nnwale efu. A na-emegharị usoro nhazi ahụ ugboro 2 ~ 3 ma were nkezi uru.
A na-agbakọ mkpokọta molar C (mol/L) nke ngwọta ọkọlọtọ sodium thiosulfate dị ka ndị a:
Ebe, M bụ uka nke potassium dichromate; V1 bụ olu sodium thiosulfate eri, mL; V2 bụ olu sodium thiosulfate riri na nnwale efu, mL; 49.03 bụ oke potassium dichromate nke dabara na 1mol nke sodium thiosulfate, g.
Mgbe nhazichara, tinye ntakịrị Na2CO3 iji gbochie ire ere microbial.
(2) Ngwọta ọkọlọtọ NaOH (0.1mol/L, nkwado: otu ọnwa)
Nkwadebe: A na-atụba ihe dịka 4.0g nke NaOH dị ọcha maka nyocha n'ime beaker, na 100mL mmiri na-ekpo ọkụ na-agbaze ka ọ gbazee, wee bufee ya na 1L volumetric flask, na-etinye mmiri na-ekpo ọkụ na ọnụ ọgụgụ, ma tinye ya maka ụbọchị 7-10 ruo mgbe. mmezi.
Nhazi: Tinye 0.6 ~ 0.8g nke potassium hydrogen phthalate dị ọcha nke a mịrị amị na 120 ℃ (zie ezie na 0.0001g) n'ime flask conical 250mL, tinye 75mL mmiri distilled ka ọ gbazee, wee tinye 2 ~ 3 tụlee nke 1% phenolphthalein na egosi, ihe ngwọta sodium hydroxide a kwadebere n'elu ruo mgbe ọ dị ntakịrị na-acha uhie uhie, na njedebe bụ na agba adịghị ada n'ime 30S. Dee olu sodium hydroxide. A na-emegharị usoro nhazi ahụ ugboro 2 ~ 3 ma were nkezi uru. Ma mee nnwale efu.
A na-agbakọ mkpokọta sodium hydroxide ngwọta dị ka ndị a:
Ebe, C bụ ntinye nke ngwọta sodium hydroxide, mol / L; M na-anọchi anya oke potassium hydrogen phthalate, G; V1 bụ olu sodium hydroxide riri, mL; V2 na-anọchi anya olu sodium hydroxide riri na nnwale efu, ml; 204.2 bụ molar mass nke potassium hydrogen phthalate, g kwa mole.
(3) Ghichaa sulfuric acid (1+9) (Ọbara: 1 ọnwa)
N'okpuru mkpali, jiri nlezianya tinye 100mL sulfuric acid concentrated na 900ml mmiri distilled, na-agbakwunye nwayọọ nwayọọ, na-akpali.
(4) Ghichaa sulfuric acid (1+16.5) (Ike ruru: ọnwa 2)
N'okpuru mkpali, jiri nlezianya tinye 100ml nke sulfuric acid gbadoro ụkwụ na 1650ml nke mmiri distilled, na-agbakwunye nwayọọ nwayọọ. Kwuo ka ị na-aga.
(5) Ihe ngosi starch (1%, nkwado: ụbọchị 30)
Were starch soluble 1.0g, tinye mmiri 10ml, kpalie ma gbanye ya n'ime mmiri esi mmiri 100ml, sie ntakịrị maka nkeji 2, tinye ya, were supernatant were were.
(6) Ihe ngosi starch
0.5% starch egosi enwetara site na-ewere 5mL nke njikere 1% starch egosi ngwọta na igbari ya na 10mL na mmiri.
(7) 30% chromium trioxide ngwọta (nke ọma: 1 ọnwa)
Were 60g nke chromium trioxide wee gbarie ya na 140ml mmiri na-enweghị ihe organic.
(8) Potassium acetate ngwọta (100g/L, irè: 2 ọnwa)
10g nke mkpụrụ osisi potassium acetate anhydrous ka agbazere na ngwọta 100ml nke 90ml glacial acetic acid na 10ml acetic anhydride.
(9) 25% sodium acetate ngwọta (220g/L, nkwado: 2 ọnwa)
Gbarie 220g nke sodium acetate anhydrous n'ime mmiri wee tụgharịa ruo 1000ml.
(10) Hydrochloric acid (1:1, nkwado: ọnwa 2)
Gwakọta hydrochloric acid na mmiri na oke 1: 1.
(11) Acetate buffer ngwọta (pH = 3.5, nkwado: ọnwa 2)
Gbarie 60mL acetic acid na mmiri 500ml, wee tinye 100ml ammonium hydroxide na itughari na 1000ml.
(12) Ngwọta nkwadebe nitrate ndu
A gbazere 159.8mg nitrate lead na mmiri 100ml nwere 1mL nke nitric acid (njupụta 1.42g/cm3), gbazere na 1000ml mmiri wee gwakọta nke ọma. A ga-eme nkwadebe na nchekwa nke ngwọta a na iko na-enweghị ndu.
(13) Ọkọlọtọ ụzọ ngwọta (nke ọma: ọnwa 2)
A na-eji mmiri gbazere nha ziri ezi nke 10mL nke ngwọta nitrate ntụ ntụ ka ọ bụrụ 100ml.
(14) 2% hydroxylamine hydrochloride ngwọta (oge nkwado: 1 ọnwa)
Gbarie 2g hydroxylamine hydrochloride na 98ml mmiri.
(15) Amonia (5mol/L, nkwado: ọnwa 2)
A na-agbaze 175.25g nke amonia na mmiri wee gbanye ya na 1000ml.
(16) Mmiri mmiri agwakọta (oge nkwado: ọnwa 2)
Gwakọta 100ml glycerol, 75mLNaOH ngwọta (1mol/L), na mmiri 25ml.
(17) Ihe ngwọta Thioacetamide (4%, nkwado: ọnwa 2)
4g thioacetamide gbazere na mmiri 96g.
(18) Phenanthroline (0.1%, nkwado: 1 ọnwa)
Gbari 0.1g o-phenanthroline na mmiri 100ml.
(19) Acid stannous chloride (nke ọma: 1 ọnwa)
Gbarie 20g stannous chloride na 50ml hydrochloric acid gbanyere mkpọrọgwụ.
(20) Potassium hydrogen phthalate ọkọlọtọ ọkọlọtọ ngwọta (pH 4.0, nkwado: 2 ọnwa)
A tụrụ 10.12g nke potassium hydrogen phthalate (KHC8H4O4) nke ọma ma kpọọ nkụ na (115±5) ℃ maka 2 ~ 3h. Wunye 1000 ml na mmiri.
(21) Ngwọta nchekwa ọkọlọtọ phosphate (pH 6.8, nkwado: ọnwa 2)
3.533g nke anhydrous disodium hydrogen phosphate na 3.387g nke potassium dihydrogen phosphate akpọnwụwo na (115±5) ℃ maka 2 ~ 3h e ziri ezi tụrụ na diluted ka 1000mL na mmiri.
3, hydroxypropyl methyl cellulose ọdịnaya mkpebi siri ike
(1) Mkpebi nke ọdịnaya methoxy
Mkpebi nke ọdịnaya methoxy dabere na nbibi nke hydroiodate acid site na kpo oku na nnwale nwere methoxy iji mepụta methane iodide na-agbanwe agbanwe (ebe isi 42.5 Celsius C). Methane iodide na-agbaze na nitrogen na ngwọta autoreaction. Mgbe ịsachara iji wepụ ihe ndị na-etinye aka (HI, I2 na H2S), ikuku methane ayodiin na-etinye uche na potassium acetate acetic acid ngwọta nwere Br2 iji mepụta IBr wee oxidized na iodic acid. Mgbe distillation gasịrị, a na-ebufe ihe ndị dị na onye na-anabata ya na karama ayodiin ma tinye ya na mmiri. Ka ịgbakwunye formic acid iji wepụ ngafe Br2, KI na H2SO4 na-agbakwunye. Enwere ike gbakọọ ọdịnaya methoxy site na titrating 12 na ngwọta nke Na2S2O3. Enwere ike igosipụta nha mmeghachi omume dịka ndị a.
Egosiri ngwaọrụ maka ịtụ ọdịnaya methoxy na eserese 7-6.
Na 7-6 (a), A bụ flask 50mL gburugburu-ala jikọtara ya na catheter. A na-eji tube na-ekpo ọkụ ikuku kwụ ọtọ, ihe dịka 25cm n'ogologo na 9mm na dayameta ime. A na-ehulata nsọtụ elu nke tube n'ime tube capillary iko nke nwere mpụta ala na dayameta 2mm n'ime. Ọgụgụ 7-6 (b) na-egosi ngwaọrụ emelitere. 1 bụ flask mmeghachi omume, nke bụ flask 50mL gburugburu, yana ọkpọkọ nitrogen dị n'aka ekpe. 2 bụ ọkpọkọ condensing kwụ ọtọ; 3 bụ scrubber, nwere mmiri ịsacha; 4 bụ tube absorption. Nnukwu ihe dị iche n'etiti ngwaọrụ na usoro pharmacopoeia bụ na a na-ejikọta ihe abụọ nke usoro pharmacopoeia n'ime otu, nke nwere ike ibelata nkwụsị nke ngwọta njedebe ikpeazụ. Tụkwasị na nke ahụ, mmiri mmiri na-asacha na scrubber dịkwa iche na usoro pharmacopoeia, nke a na-eme ka mmiri na-ekpo ọkụ, na ngwaọrụ a na-emeziwanye bụ ngwakọta nke cadmium sulfate solution na sodium thiosulfate ngwọta, nke nwere ike ime ka ihe ndị na-adịghị ọcha dị na gas distilled ngwa ngwa.
Ngwá ọrụ pipette: 5ml (5), 10ml (1); mmiri ara ehi: 50ml; Kalama nha nke iodine: 250ml; Nyochaa nguzozi.
Reagent phenol (n'ihi na ọ bụ ihe siri ike, ya mere a ga-ejikọta ya tupu nri); carbon dioxide ma ọ bụ nitrogen; Hydroiodate acid (45%); Nyocha nke dị ọcha; Potassium acetate ngwọta (100g / L); Bromine: nyocha dị ọcha; Formic acid: nyocha dị ọcha; 25% sodium acetate ngwọta (220g / L); KI: ịdị ọcha nyocha; Ghichaa sulfuric acid (1 + 9); Sodium thiosulfate ọkọlọtọ ngwọta (0.1mol / L); Phenolphthalein egosi; 1% ethanol ngwọta; Ihe ngosi starch: 0,5% starch na mmiri; Na-agbaze sulfuric acid (1 + 16.5); 30% chromium trioxide ngwọta; Mmiri na-enweghị Organic: tinye 10mL sulfuric acid (1 + 16.5) na mmiri 100 ml, kpoo ọkụ na esi, tinye 0.1ml0.02mol /L potassium permanganate titer, obụpde maka 10min, ga-edobe pink; 0.02mol/L sodium hydroxide titration ngwọta: Dị ka Chinese Pharmacopoeia appendix usoro, 0.1mol/L sodium hydroxide ngwọta a calibrated na n'ụzọ ziri ezi gbazere na 0.02mol/L na sie na mma distilled mmiri.
Tinye ihe dị ka 10mL nke ngwọta ịsacha n'ime tube ịsa ahụ, gbakwunye 31mL nke ngwọta ntinye ọhụrụ a kwadebere n'ime tube absorption, wụnye ngwá ọrụ ahụ, tụọ ihe dị ka 0.05g (nke ziri ezi na 0.0001g) nke ihe nlele a mịrị amị nke akpọnwụwo na ịdị arọ mgbe niile na 105. Tinye n'ime flask mmeghachi omume, tinye 5mL hydroiodate. A na-ejikọta karama mmeghachi omume ngwa ngwa na condenser mgbake (ọnụ na-egweri mmiri na hydroiodate), na nitrogen na-agbanye n'ime tank na ọnụego nke 1 ~ 2 bubbles kwa nkeji. A na-ejikwa nwayọọ nwayọọ na-achịkwa okpomọkụ nke mere na uzuoku nke mmiri na-esi esi na-ebili na ọkara elu nke condenser. Oge mmeghachi omume dabere na ọdịdị nke nlele ahụ, n'etiti 45min na 3h. Wepu tube nke na-amịkọrọ ahụ ma jiri nlezianya bufee ihe ngwọta na-amịkọrọ mmiri n'ime flask ayodiin 500ml nke nwere 10ml nke 25% sodium acetate ngwọta ruo mgbe mkpokọta mkpokọta ruru ihe dịka 125ml.
N'okpuru ịma jijiji mgbe niile, jiri nwayọ tinye formic acid site na dobe ruo mgbe edo edo ga-apụ n'anya. Tinye ntakịrị ihe ngosi 0.1% methyl red, na agba uhie anaghị apụ n'anya maka nkeji ise. Mgbe ahụ, tinye atọ tụlee nke formic acid. Hapụ ya n'obere oge, tinyezie 1 g nke potassium iodide na 5mL nke itule sulfuric acid (1+9). A na-eji 0.1mol/L sodium thiosulfate ọkọlọtọ ngwọta titrated ngwọta, na 3 ~ 4 tụlee nke 0.5% starch egosi na-agbakwunyere na nso njedebe njedebe, na titration gara n'ihu ruo mgbe agba anụnụ anụnụ na-apụ n'anya.
N'otu ọnọdụ ahụ, e mere nnwale efu.
Ngụkọta mkpokọta methoxide ọdịnaya:
Ebe, V1 na-anọchi anya olu (mL) nke sodium thiosulfate ọkọlọtọ ngwọta riri site titration samples; V2 bụ olu sodium thiosulfate ọkọlọtọ ngwọta riri na nnwale efu, ml; C bụ mkpokọta sodium thiosulfate ọkọlọtọ ngwọta, mol/L; M na-ezo aka n'ogo nke ihe nlele a mịrị amị, g; 0.00517 bụ 0.1mol/L sodium thiosulfate kwa 1ml dakọtara na 0.00517g nke methoxy.
Mkpokọta ọdịnaya methoxy na-anọchi anya ngụkọta methoxy yana uru hydroxyproxy nke ngụkọta methoxy, yabụ mkpokọta alkoxy ga-edozirịrị site na ọdịnaya hydroxyproxy nke na-esi na ya pụta iji nweta ọdịnaya methoxy kpọmkwem. Ọdịnaya HYDROXYPROPOXY kwesịrị ibu ụzọ dozie ya maka zie ezie na-emepụta site na mmeghachi omume nke HI na HYDROXYPROPYL na-adịgide adịgide K=0.93 (Mpụtara nke Ọnụ Ọgụgụ Morgan nke Samples Kpebie). Ya mere:
Ọdịnaya methoxy emeziri = mkpokọta methoxy ọdịnaya – (ọdịnaya hydroxypropoxy ×0.93×31/75)
Ebe ọnụọgụgụ 31 na 75 bụ oke molar nke methoxy na otu hydroxypropoxy otu, n'otu n'otu.
(2) Mkpebi nke ọdịnaya hydroxypropoxy
Otu hydropropoxy dị na nlele ahụ na-emeghachi omume na chromium trioxide iji mepụta acetic acid. Mgbe emechara ya site na ngwọta autoreaction, a na-ekpebi ọdịnaya nke chromic acid site na titration na ngwọta NaOH. N'ihi na a ga-ewepụta obere chromic acid na usoro distillation, a ga-erikwa ngwọta NaOH, ya mere, ọdịnaya nke chromic acid a ga-ekpebisi ike site na iodimetry ma wepụ ya na nchịkọta. Usoro mmeghachi omume bụ:
Ngwa na reagents Ngwa ngwa zuru oke maka ikpebi otu hydroxypropoxy; Kalama olu: 1L, 500ml; Ihe atụ cylinder: 50ml; Pipette: 10ml; Kalama nha nke iodine: 250ml. Nri bụ isi: 10ml; Sodium thiosulfate ọkọlọtọ ngwọta (0.1mol / L); Na-agbaze sulfuric acid (1 + 16.5); Ghichaa sulfuric acid (1 + 9); Ihe ngosi starch (0.5%).
7-7 bụ ngwaọrụ maka ikpebi ọdịnaya hydroxypropoxy.
Na 7-7 (a), D bụ 25mL okpukpu abụọ n'olu distilling flask, B bụ 25mm × 150mm uzuoku generator tube, C bụ a eruba njikọ tube, A bụ electric kpo oku mmanụ bath, E bụ shunt kọlụm, G bụ flask conical nke nwere plọg iko, dayameta nke dị n'ime njedebe bụ 0.25-1.25mm, tinye ya n'ime ite ọkụ; F bụ tube condensing ejikọrọ na E. Na ngwaọrụ emelitere nke egosiri na FIG. 7-7 (b), 1 bụ onye na-emepụta ihe, nke bụ 50ml distillation flask; 2 bụ isi distillation; 3 bụ oghere iko 50mL iji chịkwaa ọsọ nke mmiri mmiri organic; 4 bụ ọkpọkọ nitrogen; 5 bụ ọkpọkọ condensing. Ihe dị iche iche dị ịrịba ama n'etiti ngwaọrụ a gbanwere na usoro pharmacopoeia bụ mgbakwunye nke oghere iko iji chịkwaa ọnụ ọgụgụ mmiri na-asọba, ka ọnụ ọgụgụ nke distillation wee nwee ike ịchịkwa ngwa ngwa.
Testzọ ule na sample nke 105 ℃ ihicha ka mgbe nile arọ bụ banyere 0.1 g (0.0002 g), ezi kwuru na distillation karama, tinye 10 ml nke 30% chromium trioxide ngwọta, na distillation flask n'ime mmanụ bath iko, mmanụ bat mmiri larịị. kwekọrọ na mmiri mmiri chromium trioxide, akụrụngwa arụnyere, mmiri jụrụ oyi, nitrogen, nke ụlọ ọrụ anyị iji chịkwaa ọnụego nitrogen ihe dị ka otu afụ kwa sekọnd. N'ime 30min, mmanụ bat e kpụ ọkụ n'ọnụ ruo 155 ℃ ma nọgide na-enwe a okpomọkụ ruo mgbe anakọtara ngwọta ruru 50mL. A kwụsịrị distillation iji wepụ mmanụ bat.
Na-asa mgbidi dị n'ime nke ngwa nju oyi na mmiri distilled, jikọta mmiri ịsa ahụ na distillate na karama iodine 500mL, tinye 2 tụlee nke 1% phenolphthalide egosi, titrate na 0.02mol / L sodium hydroxide ngwọta na pH uru nke 6.9 ~ 7.1. , ma dee ngụkọta ọnụ ọgụgụ sodium hydroxide riri.
Tinye 0.5g sodium bicarbonate na 10mL dilute sulfuric acid (1+16.5) na karama ayodiin ma hapụ ya ka o guzoro ruo mgbe a naghị emepụta carbon dioxide. Mgbe ahụ, tinye 1.0g potassium iodide, gbanye ya nke ọma, gbanye ya nke ọma ma hapụ ya n'ọchịchịrị maka 5min. Mgbe ahụ, tinye 1mL 0.5% starch egosi ma titrate ya na 0.02mol/L sodium thiosulfate na njedebe njedebe. Dee olu sodium thiosulfate riri.
N'ime nnwale ọzọ efu, e dekọrọ ọnụ ọgụgụ olu sodium hydroxide na sodium thiosulfate titrator riri n'otu n'otu.
Mgbakọ nke ọdịnaya hydroxypropoxy:
Ebe, K bụ foto ọnụọgụ ngbanwe nke nnwale efu: V1 bụ olu sodium hydroxide titration nke ihe nlele ahụ riri, mL. C1 bụ mkpokọta sodium hydroxide ọkọlọtọ ngwọta, mol / L; V2 bụ olu sodium thiosulfate titration nke ihe nlele ahụ na-eri, mL; C2 bụ mkpokọta sodium thiosulfate ọkọlọtọ ngwọta, mol / L; M bụ oke nlele, g; Va bụ olu sodium hydroxide titration riri na nnwale efu, ml; Vb bụ olu sodium thiosulfate titration riri na nnwale efu, mL.
4. Mkpebi nke mmiri
Ntụle nyocha akụrụngwa (nke ziri ezi na 0.1mg); Akara karama: dayameta 60mm, elu 30mm; Na-ekpocha oven.
Usoro ule na-atụle nke ọma sample 2 ~ 4G (
Oge nzipu: Sep-08-2022